色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 908-914.DOI: 10.3724/SP.J.1123.2012.06019

• 研究论文 • 上一篇    下一篇

超高效液相色谱-电喷雾串联四极杆质谱法同时测定配合饲料中29种兽药

赵颖*, 刘瑜, 金雁, 徐宜宏, 钟钰, 蒋施, 李晓东, 曾凡, 周健南   

  1. 沈阳出入境检验检疫局综合技术中心, 辽宁 沈阳 110016
  • 收稿日期:2012-06-10 修回日期:2012-07-17 出版日期:2012-09-28 发布日期:2012-09-20
  • 通讯作者: 赵颖,硕士,高级工程师,研究方向为农兽药残留检测. Tel: (024)24812663, E-mail: zy-ciq@163.com.
  • 基金资助:

    辽宁检验检疫局科研项目(LK21-2009).

Simultaneous determination of 29 veterinary drugs in compound feeds by ultra performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry

ZHAO Ying*, LIU Yu, JIN Yan, XU Yihong, ZHONG Yu, JIANG Shi, LI Xiaodong, ZENG Fan, ZHOU Jiannan   

  1. Technology Center, Shenyang Entry-Exist Inspection and Quarantine Bureau, Shenyang 110016, China
  • Received:2012-06-10 Revised:2012-07-17 Online:2012-09-28 Published:2012-09-20

PDF

421

被引次数

49

摘要： 建立了同时测定配合饲料中喹诺酮类、磺胺类、大环内酯类和硝基呋喃类共计29种兽药的超高效液相色谱-电喷雾串联四极杆质谱(UPLC-ESI-MS/MS)检测方法。饲料样品用甲醇-乙腈(1:1, v/v)混合溶液提取,提取液经Oasis HLB固相萃取柱净化,采用UPLC-ESI-MS/MS检测。以甲醇和含0.1%(v/v)甲酸的水溶液作为流动相,进行梯度洗脱,用C18色谱柱分离,正离子模式扫描,多反应监测模式检测。29种兽药在0.01～5.0 mg/L范围内线性关系良好,相关系数(r)均大于0.99;在复合预混饲料、全价配合饲料、浓缩饲料中4个添加水平下29种兽药的平均回收率在61.2%～94.3%范围内,相对标准偏差(RSD)为2.2%～15.0%;方法的检出限(以信噪比大于10计)为0.01 mg/kg或0.05 mg/kg。该方法简便、快速、准确,重现性好,灵敏度高,适用于配合饲料中多种兽药的同时检测。

关键词: 超高效液相色谱-电喷雾串联四极杆质谱, 配合饲料, 兽药

Abstract: An ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed for the simultaneous determination of 29 veterinary drugs of quinolones, sulfonamides, macrolides and nitrofurans in compound feeds. The sample was extracted with methanol-acetonitrile (1:1, v/v), and then cleaned up using solid phase extraction with an Oasis HLB column, detected by UPLC-ESI-MS/MS. The UPLC separation was performed on a C18 column (100 mm×2.1 mm, 1.7 μm) using a gradient elution with the mobile phases of methanol and 0.1% (v/v) formic acid aqueous solution. The ESI-MS/MS detection was achieved in positive mode under multiple reaction monitoring (MRM) mode. The linear ranges were from 0.01 to 5.0 mg/L with the correlation coefficients above 0.99 for all the 29 veterinary drugs. The average recoveries of the 29 veterinary drugs spiked in three feed matrixes (the compound premix feed, the complete formula feed and the concentrated feed) at four spiked levels were 61.2%~94.3% with the relative standard deviations (RSDs) of 2.2%~15.0%. The limits of detection were 0.01 mg/kg or 0.05 mg/kg. The method is rapid, accurate, reproducible, sensitive and easy to apply, and suitable for the simultaneous determination of diverse veterinary drugs in compound feeds.

Key words: compound feeds, veterinary drugs, ultra performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry (UPLC-ESI-MS/MS)